Standard Test Method for Density, Relative Density, and AP! Gravity of Liquids by Digital Density Meter’ “This standard is issued under the fixed desigaation D40S2; the mimher immediately folowing the designation indicates the year of original agepton on the cae of reviion, the gent of last evsion. A mer x paentier infest: the yar of last roapproval A supersenp etn (e) neat an eval change sine the ls revision or reaper. This stant has been approved for use y agencies ofthe US. Department of Defense. 1. Seope® 1.1 This test method covers the determination of the density, relative density, and API Gravity of petroleum distillates and ‘viscous oils that can be handled in a normal fashion as liquids at the temperature of test, utilizing either manual or automated sample injection equipment. Its application is restricted to liquids with total vapar pressures (see Test Method DS191) typically below 100 kPa and viscosities (see Test Method D445 ‘or D7042) typically below about 15 000 mm/s atthe tempera ‘ture of test. The total vapor pressure limitation however can be extended to >100 kPa provided that it is first ascertained that rno bubbles form in the U-shaped, oscillating tube, which can affect the density determination. Some examples of products that may be tested by this procedure include: gasolune and gasoline-oxygenate blends, diesel, jet, basestocks, waxes, and Iubricating oils. L.L.1 Waxes and highly viscous samples wee not included in the 1999 interlaboratory study (ILS) sample set that was used to determine the current precision statements of the method, since all samples evaluated at the time were analyzed ‘ta test temperature of 15 °C, Wax and highly viscous samples require a temperature cel] operated at elevated temperatures necessary to ensure a liquid test specimen is introduced for analysis, Consult instrument manufacturer instructions for appropriate guidance and precautions when attempting to ‘analyze wax or highly viscous samples. Refer to the Precision ‘and Bias section of the method and Note 8 for more detailed information abcut the 1999 ILS that was conducted. 1.2 In cases of dispute, the releree method isthe one where samples are introduced manually as in 6.3 or 6.4, as appropri- ate for sample type. 1.3 When testing opaque samples, and when not using ‘equipment that is capable of automatic bubble detection, proper procedure shall be established so that the absence of air This est rae) is unser the jualicion of ASTM. Cone DO? on Pgeents Pret, Lig Foes an Llvicaats a he dec esposilsy of ‘Subcormulice DO2O4D on Physical an Chemical Methods CCrtet edition approved Dec. 1, 2016. Pablsbed January 2017. Originaly apgeoved in 1981. La previ edion aprovad in 2015 as D4052 15. DOE 191s201082-16, bubbles in the sample cell can be established with certainty For the determination of density in erude cil samples use Test Method D5002. 1.4 The values stated in SI units are regarded as the standard, unless stated otherwise. The accepted units of mea- sure for density are grams per millltre (g/ml) or kilograms per cubic metre (kg/n®) 1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appro- priate safety and health practices and determine the applica- Dility of regulatory limitations prior 10 use. For specific warming statements, see 7.4, 7.5, and 10.3. 2. Referenced Documents 21 ASTM Standards: D287 Test Method for API Gravity of Crude Petroleum and Petroleum Products (Hydrometer Method) D445 Test Method for Kinematic Viscosity of Transpsrent and Opaque Liquids (and Calculation of Dynamic Viscos- ity) 1D1193 Specification for Reagent Water 11250 Guide for Use of the Petroleum Measurement Tables 11298 Test Method for Density, Relative Density, or API Gravity of Crude Petroleum and Liquid Petroleum Prod- ucts by Hydrometer Methiod 4057 Practice for Manual Sampling of Petroleum and Petroleum Products D417 Practice for Automatic Sampling of Petroleum and Petroleum Procucts| 1D4377 Test Method for Water in Crude Oils by Potentiomet- ric Karl Fischer Titration 15002 Test Method for Density and Relative Density of ride Oils by Digital Density Analyzer D5I91 Test Method for Vapor Pressure of Petroleum Prod- ucts (Mini Method) or referenced ASTM stanly he ASTM wetse, wwwasunceg. ce ‘contact ASTAE Customer Service at senine more. Fo ia Boot of AST ‘Standards vase information, eer oth stands Doce Stay page 08 the ASTM webs,df] Daosa - 16 ‘D7042 Test Method for Dynamic Viscosity and Density of, Liguids by Stabinger Viscometer (and the Calculation of Kinematic Viscosity) 3. Terminology 3.1 Definitions: 3.1.1 density, n—mass per unit volume at a specified tem- perature, 3.1.2 relative density, n—the ratio of the density of a material at a stated temperature to the density of water at a stated temperature. 3.2 Definitions of Terms Specific to This Standard: 3.2.1 adjustment, y—the operation of bringing the instru- ment to astate of performance suitable for its use, by setting ot adjusting the density meter constant. 3.2.1.1 Diseussion—On some digital density analyzer instruments, an adjustment may be made rather than calibrating the instrument. The adjustment procedure uses ait and freshly boiled reagent water (Warning—Handling water at boiling or near boiling temperature can present a safety hazard. Wear appropriate: personal protective equipment.) as standards to establish the linearity of measurements over a range of ‘operating temperatures. 3.2.2 calibration, v—set of operations that establishes the telationship between the reference density of standards and the corresponding density reading of the instrument. 4. Summary of Test Method. 4.1 A small volume, approximately 1 mL. to 2 ri, of liquid sample is introduced into an oscillating sample tube and the change in oscillating frequency caused by the change in the mass of the tube is used in conjunction with calibration data to determine the density, relative density, or API Gravity of the sample. Both manual and automated injection techniques are deseribed, 5. Signifleance and Use 5.1 Density is a fundamental physical property that can be used in conjunction with other properties to characterize both, the light and heavy fractions of petroleum and petroleam products, 5.2 Determination of the density ot relative density of petroleum and its products is necessary for the conversion of measured volumes to Volumes at the standard temperature of 15°C. 6. Apparatus 6.1 Digital Density Analyzer—A digital analyzer consisting of a U-shaped, oscillating sample tube and a system for electronic excitation, frequency counting, and display. The analyzer shall accommodate the accurate measurement of the ‘sumple temperature during measurement or shall control the ‘sample temperature as described in 6.2, The instrument shall be capable of meeting the precision requirements described in this test method, 6.2 Circulating Constant-Temperature Bath, (optional), ca- pable of maintaining the temperature of the circulating liquid constant to +0.05 °C in the desired range. Temperature control can be maintained as part of the density analyzer instrument package. 6.3 Syringes, for use primarily in manual injections, at least ‘2m in volume with a tip or an adapter tip that will it the opening of the oscillating tube. 64 Flow-Through or Pressure Adapter, for use as an alter- native means of introdueing the sample into the density analyzer either by a pump, by pressure, or by vacuum, Nore 1—It is highly recommended that a vacuum not be applied to samples prone to fight end lose, as itcan easily lead to the formation of bobs. tis recommenced to fabricate a special cap or stopper for sample ‘containers so tha ai, suchas from a sguceze pump. is wed t displace a test specimen to the U-tube measuring cell by the fiow-throogh method 6.5 Antosampler, required for use in automated injection analyses. The autosampler shall be designed to ensure the integrity of the test specimen pricr to and curing the analysis, and be equipped to transfer a representative portion of test specimen to the digital density analyzer. 6.6 Temperature Sensing Device (TSD), capable of monitor- ing the observed test temperature to within an accuracy of + 0.05 °C. Ifa liquic-in-glass thermometer is used as the TSP, itshall be calibrated and graduated to 0.1 °C, and have a holder that can be attached to the instrument for setting and observing, the test temperature. In calibrating the thermometer, the ice point and bore connections should be estimated to the nearest 0.05 °C. For non-mereurial thermometers, the TSD device shall be calibrated at least annually against a certified and traceable standard 6. Ultrasonic Bath, Unheated, (optional), of suitable di- ‘mensions to hold container(s) placed inside of bath, for use in effectively dissipsting and removing air ot gas bubbles that ‘may be entrained in viscous sample types prior to analysis. 7, Reagents and Materials 7.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Commit- tee on Analytical Reagents of the American Chemical Society, where such specifications are available.” Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high parity to permit its use without lessening the accuracy of the determination. 1.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water as defined by Type II of Specification D1193 or higher. 7.3 Water reagent water, freshly boiled to remove dissolved gasses, for use as primary calibration standard. (Warning— Handiing water st boiling ot near boiling temperature ean present a safety hazard. Wear appropriste personal protective equipment.) Reagent Chemists, American Chemical Society Speciation, Amwticn Ccheneat Sole, Wathiagon, DC. Far stggeitons othe esting of reagents not listed by the Amecan Chemical Society, se Analar Standards for Laboratory Chanieats, BDH Lid, Poole, Deset U.K. and the Unéed Sats Pharmacopeia and National Formers, US. Pharmscatcal Conveatio, Inc, (USPC), Recki, MD.df] Daosa - 16 7.4 Cleaning Solvent, such as petroleum naphtha* (Warning—Petroteum naphtha is extremely flammable), ot other materials that are capable of flushing and removing samples entirely from the sample tube. 75S Acetone, for flushing and drying the sample tube. (Warning—Extremely flammable.) 7.6 Dry Air, for drying the oscillator tube 8, Sampling, Test Specimens, and ‘Test Units 8.1 Sampling is defined as all the steps required to obtain an. aliquot of the contents of any pipe, tank, or other system, and to place the sample into the laboratory test container. The laboratory test container and sample volume shall be of sulficient capacity to mix the sample and obtain a homoge ‘neous sample for analysis. 8.2 Laboratory Sample—Use only representative samples ‘obtained as specified in Practices 4057 or D4177 for this test method, 83 Test Specimen—A portion or volume of sample obtained, from the laboratory sample and delivered to the density analyzer sample tube. The test specimen is obtained as follows: 8.3.1 Mix the sample if required to homogenize, taking care to avoid the introduction of air bubbles. The mixing may be accomplished as described in Practice D4177 or Test Method D437, Mixing at room temperature in an open containervan result in the loss of volatile material from certain sample types (For example, gasoline samples), so mixing in closed; pressur- ized containers or at least 10 °C below ambient temperature is required for such sample types where loss of volatile material is a potential concer. For some sample types, sich as viscous lube oils that are prone to having entrained air or gas bubbles present in the sample, the use of an ultrasonic bath (see 6.7) ‘without the heater turned on (if so equipped), has been found effective in dissipating bubbles typically within 10 min None 2—When mixing samples with volatile components, consider the sample properties in relation to both arbicat temperature and pressure, 8.3.2 For manual injections, draw the test specimen from a properly mixed laboratory sample using an appropriate sy- ringe. IF the proper density analyzer attachments and connect ing tubes are used, as described in 6.4, then the test specimen ‘ean be delivered directly to the analyzet’s sample tube from the mixing container. For automated injections, it is necessary 10 first transfer a portion of sample by appropriste means from a properly mixed laboratory sample to the autosampler vials, and take the necessary steps to ensure the integrity of the test specimen prior to and during the analysis. Sample vials for the autosampler shall be sealed immediately after filling up to 80% + S% and shall be kept closed until the auto sampler transfers the test specimen into the measuring cell. For highly volatile samples, cool the sample prior to measurement, Follow the manufacturer's instructions. Nore 3Overfilled sample vials can result in cross contamination between sample vials “Stable solvent mplthas are marketed unicr various designitons sch a= “Pecoleam Be." “Litoing” ce “Precipitation Napa” 9, Preparation of Apparatus 9.1 Set up the density analyzer (including the constant temperature bath and related attachments, if necessary) follow- ing the manufacturer's instructions. Adjust the bath or internal tempersture control so that the desired test temperature is, established snd maintained in the sample compartment of the analyzer, Calibrate the instrument at the same temperature at which the density or relative density of the sample is to be ‘measured or perform an adjustment (see 3.2.1—Discussion) in preparation of analyzing samples. (Warning—Precise setting and control of the test temperature in the sample tube is extremely important. An error of 0.1 °C can result in a change in density of one in the fourth decimal when measuring in units of grams per milllitre.) 10. Calibration of Apparatus 10.1 As a minimum requirement, calibration of the instru- ‘ment is required when first set up, whenever the test tempera ture is changed (unless the instrament is capable of performing an adjustment; see 3,2.1 Discussion), or as dictated by quality control (QC) sample results (see 11.1). 10.2 When calibration of the instrument is required, it is necessary to calculate the values of the constants A and B from the periods of cscillation (7) observed when the sample cell contains air and freshly boiled (Warning—Handling water at boiling or near boiling temperature can present a safety hazard. ‘Wear appropriate personal protective equipment.) reagent wa- tet. Other calibrating materials such as n-nonane, n-tridecane, cyclohexane, and n-hexadecane (for high temperature applica- tions) can also be used as appropriate, provided the reference ‘materials have density values that are certified and traceable to national standards, Nove 4—On certain newer, commercially available instruments, viseosiy conection feature may be available and uilzed in density determinations to minimize potential biases, Refer o information inthe Section 15 for mow species 10.2.1 While monitoring the oscillator period, 7, flush the sample tube with cleaning solvent, followed with an acetone flush and dry with cry ait. Contaminated or humid air can affect the calibration, When these conditions exist in the laboratory, pass the air used for calibration through a suitable purification and drying train. In addition, the inlet and outlet ports for the Uctube must be plugged during measurement of the calibration, ait to prevent ingress of moist air. 10.2.2 Allow the dry air in the U-tube to come to thermal equilibrium with the test temperature and record the T-value for ait 10.2.3 Introduce a small volume, about 1 mL to 2 mL, of freshly boiled (Warning—Handling water at boiling or near boiling temperature can present a safety hazard. Wear appro- priate personal protective equipment.) reagent water into the sample tube using a suitable syringe or altemate, as described in 6.4 and 6,5. The test portion must be homogeneous and free of even the smallest air or gas bubbles. Allow the display to reach a steady reading and record the T-value for water. 10.24 Calculate the density of air at the temperature of test using the following equation: